CN113075147B - Sasa class magnesium metal organic complex material, preparation method thereof and application of material in detecting sulfur-containing malodorous substances - Google Patents

Sasa class magnesium metal organic complex material, preparation method thereof and application of material in detecting sulfur-containing malodorous substances Download PDF

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CN113075147B
CN113075147B CN202110222799.9A CN202110222799A CN113075147B CN 113075147 B CN113075147 B CN 113075147B CN 202110222799 A CN202110222799 A CN 202110222799A CN 113075147 B CN113075147 B CN 113075147B
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ciprofloxacin
metal organic
organic complex
magnesium metal
solution
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CN113075147A (en
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刘刚
李挺
李毅楠
张菩
肖雅文
张博文
于文晗
单昕岚
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Nankai University Binhai College
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light

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Abstract

The invention discloses a sars magnesium metal organic complex material, a preparation method thereof and application of detecting sulfur-containing malodorous substances, wherein 0.01-0.25 mmol/L ciprofloxacin solution and 0.5-1 mol/L magnesium salt solution are respectively prepared, and the ciprofloxacin solution comprises the following components in percentage by volume: the magnesium salt solution is (10-20): 1, controlling the two solutions to be below 50 ℃ respectively, carrying out ultrasonic treatment for 30 minutes, slowly adding a magnesium salt solution into a ciprofloxacin solution, stirring at a constant speed of 60rpm for 2-3 hours, filtering to remove impurities, and standing at a low temperature of 4 ℃ for more than 15 days for natural crystallization to obtain a white solid; and (3) after the white solid is not increased any more, vacuumizing and filtering, and drying the white solid in an oven at the temperature of below 80 ℃ to finally obtain the ciprofloxacin magnesium metal organic complex. Solves the problems of complex operation steps, expensive instruments, short storage time of detection reagents, harsh detection conditions and the like in the detection of the sulfur-containing malodorous organic pollutants.

Description

Sasa class magnesium metal organic complex material, preparation method thereof and application of material in detecting sulfur-containing malodorous substances
Technical Field
The invention belongs to the technical field of environmental detection, and particularly relates to a sars magnesium metal organic complex material, a preparation method thereof and application of the sars magnesium metal organic complex material in detection of sulfur-containing malodors.
Background
The sulfur-containing substances are the main sources of common malodor influencing factors in the environment, can directly enter a human body through volatilization and diffusion, and can also release toxic malodorous gases into respiratory tracts after decomposition and conversion to cause respiratory diseases of the human body, such as allergy, nausea and the like. Excessive sulfur-containing compounds can cause pathological changes in human bodies to cause dyskinesia, and if the sulfur-containing compounds are in an environment polluted by sulfur-containing malodorous odors for a long time, cells of nasal mucosa and lung tissues can be damaged, allergic cold and fever can be caused, and brain tissues can be damaged, and malignant diseases such as tumors and cancers can be caused. Therefore, the strict monitoring of the existence of the substances in the environment, especially the emission concentration of the malodorous substances in the surrounding environment of enterprises for producing and discharging the sulfur-containing substances, is very important for timely treatment and rectification, and is beneficial to the environmental protection and the health safety guarantee of people.
The existing methods for detecting sulfur-containing malodorous substances mainly comprise liquid chromatography, gas chromatography, three-point olfactory discrimination and the like, and have the defects of complex operation, long analysis time, difficult storage of detection reagents or high requirements of detectors and the like, so that the finding of an indicator capable of efficiently, quickly and simply detecting the sulfur-containing malodorous substances in the environment and the establishment of a related detection method are a difficulty in the field of environmental monitoring.
The metal organic complex has the advantages of rich varieties, various structures, outstanding performance and the like, and has wide application prospects in the fields of sensing detection, organic matter adsorption and separation, heterogeneous catalysis, photoelectric conversion and the like. The specific metal organic complex is used as a molecular probe, can efficiently identify pollutant factors in the environment, such as metal ions, volatile gases, organic matter micromolecules and the like, and has the characteristics of quick reaction, convenient application, easy storage, low cost and the like.
Disclosure of Invention
The invention aims to solve the technical problems of providing a sars magnesium metal organic complex material, a preparation method thereof and application of the sars magnesium metal organic complex material in detecting sulfur-containing malodorous substances, and solving the problems of complex operation steps, expensive instruments, short storage time of detection reagents, harsh detection conditions and the like in detecting sulfur-containing malodorous organic pollutants.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a sars magnesium metal organic complex material comprises the steps of preparing 0.01-0.25 mmol/L ciprofloxacin solution and 0.5-1 mol/L magnesium salt solution respectively, and preparing the ciprofloxacin solution according to the volume ratio: the magnesium salt solution is (10-20): 1, controlling the two solutions to be below 50 ℃ respectively, carrying out ultrasonic treatment for 30 minutes, slowly adding a magnesium salt solution into a ciprofloxacin solution, stirring at a constant speed of 60rpm for 2-3 hours, filtering to remove impurities, and standing at a low temperature of 4 ℃ for more than 15 days for natural crystallization to obtain a white solid; and (3) after the white solid is not increased any more, vacuumizing and filtering, and drying the white solid in an oven at the temperature of below 80 ℃ to finally obtain the ciprofloxacin magnesium metal organic complex.
The ultrasonic power is kept at 0.3-0.5W/cm 2 And the ultrasonic frequency is 30-50 KHz.
The sars magnesium metal organic complex material prepared by the preparation method.
The application of the sars magnesium metal organic complex material prepared by the preparation method in detecting sulfur-containing malodorous substances.
The invention has the beneficial effects that: based on an organic complex synthesized by ciprofloxacin and magnesium salt, various sulfur-containing malodorous organic substances can be detected by utilizing the negative linear correlation between the ultraviolet absorption value of the complex and the concentration of malodorous substances under the characteristic wavelength. The method is simple, low in cost and mild in reaction condition. The organic complex has low detection lower limit on various sulfur-containing malodorous substances, strong sensitivity and good stability, can be stored for a long time at normal temperature, and is easier to store and carry than detection reagents used in the existing malodorous substance detection methods, so the organic complex can also be used for developing related malodorous substance detection kits.
Drawings
FIG. 1 is a structural view of an infrared spectrum of a ciprofloxacin raw material and a ciprofloxacin magnesium metal complex sample;
FIG. 2 is a structural diagram of a ciprofloxacin magnesium complex provided by the invention
FIG. 3 is a scanning ultraviolet-visible spectrum of a 1mmol/L aqueous solution of a sample of a ciprofloxacin magnesium metal complex prepared according to the present invention;
FIG. 4 is a diagram showing the detection of ultraviolet absorption at 235nm of sulfanilic acid at different concentrations by using the ciprofloxacin magnesium complex provided in example 2 of the present invention as a probe;
FIG. 5 is a 235nm UV absorption test chart of ciprofloxacin magnesium complex provided in example 3 as a probe against cysteine at different concentrations.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preparation method of the sars magnesium metal organic complex material comprises the following steps of respectively preparing 0.01-0.25 mmol/L ciprofloxacin solution and 0.5-1 mol/L magnesium salt solution, wherein the ciprofloxacin solution comprises the following components in percentage by volume: the magnesium salt solution is (10-20): 1, controlling the two solutions to be below 50 ℃ respectively, carrying out ultrasonic treatment for 30 minutes, slowly adding a magnesium salt solution into a ciprofloxacin solution, stirring at a constant speed of 60rpm for 2-3 hours, filtering to remove impurities, and standing at a low temperature of 4 ℃ for more than 15 days for natural crystallization to obtain a white solid; and (3) after the white solid is not increased any more, vacuumizing and filtering, and drying the white solid in an oven at the temperature of below 80 ℃ to finally obtain the ciprofloxacin magnesium metal organic complex.
The ultrasonic power is kept at 0.3-0.5W/cm 2 And the ultrasonic frequency is 30-50 KHz.
The sars magnesium metal organic complex material prepared by the preparation method.
The application of the sars magnesium metal organic complex material prepared by the preparation method in detecting sulfur-containing malodorous substances.
The sample of the complex is prepared by adopting an infrared spectrometer at 400-4000cm -1 In the range, an infrared spectrogram is measured on a Bruker VERTEX70 Fourier transform infrared spectrometer by a KBr tablet pressing method (see figure 1, CIF is ciprofloxacin, and CIF-Mg is the prepared ciprofloxacin magnesium metal organic complex).
The infrared spectrogram of the sample is analyzed, and meanwhile, the analysis of the structure of the Cu complex by Iztok Turel and the like is used for reference. Two possible structural formulas of the sars magnesium metal organic complex are shown in figure 2(X is an anion of a magnesium salt)
The prepared 1mmol/L aqueous solution of the ciprofloxacin magnesium metal organic complex is scanned under the ultraviolet and visible spectrums of 190nm to 1100nm, as shown in figure 3, the solution has stronger absorption in the ultraviolet spectrum region of 190nm to 350nm (possibly, the absorption is lower than 190 nm), wherein, the strongest absorption peak is arranged near 235nm, and the common ultraviolet absorption detection spectrum (not limited to the value) for detecting sulfur-containing malodorous organic matters as the complex is provided
The test materials and reagents used in the following examples, etc., are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
Preparing a ciprofloxacin magnesium complex: respectively preparing 100mL of 0.25mmol/L ciprofloxacin solution and 1L of 0.8mol/L magnesium sulfate aqueous solution, controlling ultrasonic waves (ultrasonic power is kept at 0.3-0.5W/cm 2, ultrasonic frequency is 30-50 KHz) at 40 ℃ for 30 minutes, slowly adding the magnesium sulfate solution into the ciprofloxacin solution, uniformly stirring at 60rpm for 3 hours, filtering to remove impurities, and standing at the low temperature of 4 ℃ for 15 days to obtain white solid; and (3) after the white solid is not increased any more, vacuumizing and filtering, and drying the white solid in an oven at 75 ℃ to finally obtain the ciprofloxacin magnesium metal organic complex.
Example 2
Application of ciprofloxacin magnesium complex in detecting concentration of sulfanilic acid (sulfur-containing organic matter)
The prepared ciprofloxacin magnesium metal organic complex 1mmol/L water solution is added with sulfanilic acid until the final concentration is respectively 0.05g/L, 0.1g/L, 0.15g/L, 0.2g/L and 0.25g/L, and the absorbance value is measured under 235nm ultraviolet absorption, as can be seen in figure 4, under the condition of low concentration, the ultraviolet absorption value of the solution is reduced in a linear trend along with the increase of the concentration of sulfanilic acid, and the content of sulfanilic acid in a sample can be measured in a certain range.
Example 3
Application of ciprofloxacin magnesium complex in detecting concentration of cysteine (sulfur-containing organic matter)
The prepared 1.5mmol/L aqueous solution of the ciprofloxacin magnesium metal organic complex is added with cysteine until the final concentration of the solution is respectively 0.5g/L, 1g/L, 1.5g/L, 2g/L and 2.5g/L, and the absorbance value is measured under 235nm ultraviolet absorption, as shown in figure 5, under the condition of low concentration, the ultraviolet absorption value of the solution is reduced in a linear trend along with the increase of the concentration of the cysteine, and the content of the cysteine in a sample can be measured in a certain range.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (2)

1. The application of a sars magnesium metal organic complex material in detecting malodorous substances containing sulfanilic acid or cysteine;
the preparation method of the sars magnesium metal organic complex material comprises the following steps: respectively preparing 0.01-0.25 mmol/L ciprofloxacin solution and 0.5-1 mol/L magnesium salt solution, wherein the ciprofloxacin solution comprises the following components in percentage by volume: the magnesium salt solution is (10-20): 1, controlling the two solutions to be below 50 ℃ respectively, carrying out ultrasonic treatment for 30 minutes, slowly adding a magnesium salt solution into a ciprofloxacin solution, stirring at a constant speed of 60rpm for 2-3 hours, filtering to remove impurities, and standing at a low temperature of 4 ℃ for more than 15 days for natural crystallization to obtain a white solid; and (3) after the white solid is not increased any more, vacuumizing and filtering, and drying the white solid in an oven at the temperature of below 80 ℃ to finally obtain the ciprofloxacin magnesium metal organic complex.
2. The application of the sars magnesium metal organic complex material in detecting malodorous substances containing sulfanilic acid or cysteine according to claim 1, wherein the ultrasonic power is kept at 0.3-0.5W/cm 2 And the ultrasonic frequency is 30-50 KHz.
CN202110222799.9A 2021-02-26 2021-02-26 Sasa class magnesium metal organic complex material, preparation method thereof and application of material in detecting sulfur-containing malodorous substances Active CN113075147B (en)

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AU2003261038A1 (en) * 2002-06-27 2004-01-19 Robert Janitzek Ciprofloxacin hci
CN100445731C (en) * 2004-11-12 2008-12-24 中国科学院兰州化学物理研究所 Method for colorimetric detecting and analysing cysteine
GB0912744D0 (en) * 2009-07-22 2009-08-26 Imp Innovations Ltd Methods and uses
CN101672792B (en) * 2009-09-22 2012-01-11 广东省药品检验所 Detection method of quinolone drugs, detection reagent kit and application
CN103288857B (en) * 2013-06-08 2015-09-30 山东理工大学 Sarafloxacin metal complex and preparation method thereof
CN104288112A (en) * 2014-09-30 2015-01-21 地奥集团成都药业股份有限公司 Levofloxacin hydrochloride tablets
CN107141255A (en) * 2017-06-19 2017-09-08 广西师范大学 Enrofloxacin calcium chelate and its synthetic method and application
JPWO2020129509A1 (en) * 2018-12-21 2021-11-04 富士フイルム株式会社 Methods for measuring phototoxicity or photoallergy and reagents for use in the above measuring methods
CN110463719A (en) * 2018-12-29 2019-11-19 黑龙江大学 Ciprofloxacin metal complex-polyalkenylalcohols compound and its preparation method and application

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